CN101481090A - Preparation method of sodium percarbonate - Google Patents
Preparation method of sodium percarbonate Download PDFInfo
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- CN101481090A CN101481090A CNA2009100953961A CN200910095396A CN101481090A CN 101481090 A CN101481090 A CN 101481090A CN A2009100953961 A CNA2009100953961 A CN A2009100953961A CN 200910095396 A CN200910095396 A CN 200910095396A CN 101481090 A CN101481090 A CN 101481090A
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- hydrogen peroxide
- suspension
- spc
- preparation
- sodium percarbonate
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 title abstract description 9
- 229940045872 sodium percarbonate Drugs 0.000 title abstract description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000000725 suspension Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012452 mother liquor Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 230000032683 aging Effects 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 238000005185 salting out Methods 0.000 claims description 15
- 235000017550 sodium carbonate Nutrition 0.000 claims description 15
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 15
- 150000005846 sugar alcohols Polymers 0.000 claims description 15
- 235000019353 potassium silicate Nutrition 0.000 claims description 14
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 claims description 12
- 229940051250 hexylene glycol Drugs 0.000 claims description 12
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 10
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims description 10
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 7
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 7
- 159000000003 magnesium salts Chemical class 0.000 claims description 7
- 238000002203 pretreatment Methods 0.000 claims description 7
- 150000003016 phosphoric acids Chemical class 0.000 claims description 6
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 5
- 239000011654 magnesium acetate Substances 0.000 claims description 5
- 235000011285 magnesium acetate Nutrition 0.000 claims description 5
- 229940069446 magnesium acetate Drugs 0.000 claims description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 5
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 5
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 5
- 239000001488 sodium phosphate Substances 0.000 claims description 5
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 5
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 5
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 5
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 5
- 239000004111 Potassium silicate Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 4
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 4
- 239000000084 colloidal system Substances 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 abstract description 6
- 230000012010 growth Effects 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract 2
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 230000005484 gravity Effects 0.000 abstract 1
- 239000010413 mother solution Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000008187 granular material Substances 0.000 description 3
- 230000007773 growth pattern Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 101100433727 Caenorhabditis elegans got-1.2 gene Proteins 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000006213 oxygenation reaction Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- -1 phospho Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 150000004291 polyenes Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- MSLRPWGRFCKNIZ-UHFFFAOYSA-J tetrasodium;hydrogen peroxide;dicarbonate Chemical compound [Na+].[Na+].[Na+].[Na+].OO.OO.OO.[O-]C([O-])=O.[O-]C([O-])=O MSLRPWGRFCKNIZ-UHFFFAOYSA-J 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Detergent Compositions (AREA)
Abstract
The invention discloses a method for preparing sodium percarbonate, which comprises preparing a suspension a and a mother solution b; aging to separate out sodium percarbonate crystals, and performing solid-liquid separation. In the preparation of the mother liquor b, the way of respectively adding the floating liquor a and hydrogen peroxide into the reactor is as follows: and the suspension a and the hydrogen peroxide solution are simultaneously dripped into the reaction kettle. The hydrogen peroxide added in the step B is pretreated, and the pretreatment of the hydrogen peroxide is as follows: adding the oligomeric alcohol into hydrogen peroxide with the mass percentage concentration of 25-50%, wherein the addition amount of the oligomeric alcohol is 0.05-1.0% of the mass of the hydrogen peroxide. By adopting the scheme, the growth mode of the sodium percarbonate is an agglomeration type, and the crystallized sodium percarbonate particles are loose and have lighter specific gravity, and the dissolution speed and the stability are improved compared with those of the common crystallized sodium percarbonate.
Description
Technical field
The present invention relates to a kind of preparation method of SPC-D, the method for a kind of SPC-D wet production of more specifically saying so belongs to the inorganic peroxide preparing technical field of oxygen-bearing bleaching agent.
Background technology
SPC-D has another name called sodium carbonate peroxide, is called for short SPC, and its molecular formula is 2Na
2CO
33H
2O
2, molecular weight is 314.02, and theoretical oxygen level is 15.28%, its physical properties aspect shows as the particulate state or the powdered crystal of white, loose, good fluidity, and nontoxic, tasteless, soluble in water.Its character not only makes it have the bleaching function, also having functions such as sterilization, sterilization, decontamination, is fields such as washing powder, soap powder, chlorinated lime, dyeing and finishing agent, boil off agent, food sanitizer and fruit freshness preserving, pond oxygenation thereby make it be widely used in oxygen.
In prior art was open, the preparation SPC-D mainly was dry production and two kinds of methods of wet production.The SPC-D epigranular that dry method production process obtains is convenient to parcel, and stability is preferably arranged, and raw material consumption is low simultaneously.But this method is had relatively high expectations to using on raw material and the equipment.
The wet production characteristics are reacted in solution exactly, at first oversaturated suspension of preparation of raw material such as yellow soda ash, salting-out agent, stablizers, and then in certain sequence hydrogen peroxide solution and suspension are joined in the reactor, in reactor, yellow soda ash and hydrogen peroxide are through constantly reaction, the continuous crystallization of sodium percarbonate granules is separated out under the effect of salting-out agent simultaneously, just can obtain sodium percarbonate granules through centrifugal, drying course again.This method technology, equipment are simple.
In the wet production, the general stablizer that adopts is respectively silicate, solubility magnesium salts, organic phospho acid and salt, ethylenediamine tetraacetic acid (EDTA) and salt thereof, polyene hydrochlorate etc. now, and salting-out agent generally adopt soluble sodium salt such as sodium sulfate, sodium-chlor etc.But there is certain defective wet in it aspect stable the SPC-D of this method preparation, has used oligomeric alcohols material in the stablizer of the present invention, has improved the character of crossing the carbon this respect to a certain extent greatly.
The wet process technique of SPC-D mainly be to rely on crystallization to separate out, and SPC-D mainly contains two kinds of growth patterns at crystallisation process: reunion crystallization and self-sow crystallization simultaneously.General wet production process, the growth pattern of SPC-D all is a self-sow, and graininess is more solid, and proportion is heavier, and stable aspect is general.
Summary of the invention
The invention provides a kind of preparation method that can effectively improve dissolution rate, improve the SPC-D of the wet stability of product.
For achieving the above object, the present invention has adopted following technical scheme: a kind of preparation method of SPC-D, and it may further comprise the steps:
A: yellow soda ash, salting-out agent, stablizer are mixed, be mixed with suspension a, described weight ratio with yellow soda ash, salting-out agent, stablizer is 1:0.1-0.8:0.01-0.05;
B: suspension a and hydrogen peroxide are added respectively in the reactor, and the volume ratio of described suspension a and hydrogen peroxide is 1:1-3, obtains mother liquor b;
C: with mother liquor b ageing 5-10 minute;
D: separate out the SPC-D crystal,, the solid drying after separating is obtained the finished product SPC-D through solid-liquid separation,
At salting-out agent described in the steps A is sodium-chlor or sodium sulfate, and described stablizer is silicate, solubility magnesium salts, phosphoric acid salt,
Among the described step B, the mode that suspension a and hydrogen peroxide are added respectively in the reactor is: described suspension a and hydrogen peroxide solution are simultaneously in the dropwise reaction still.
The hydrogen peroxide that adds among the described step B is for through pre-treatment, and the pre-treatment of described hydrogen peroxide is: add low polyalcohols in mass percentage concentration is the hydrogen peroxide of 25%-50%, the add-on of described low polyalcohols is the 0.05-1.0% of hydrogen peroxide quality.
The low polyalcohols that adds in the described hydrogen peroxide is any one or more mixture of poly-hexylene glycol or poly-hexanol or poly-hexylene glycol.Rate of addition in described suspension a and the hydrogen peroxide solution while dropwise reaction still is: the volume ratio 1:1-3 of suspension a and hydrogen peroxide solution, the dropping time in described suspension a and the hydrogen peroxide solution while dropwise reaction still is 30-50 minute.
In the described steps A, when being mixed with suspension a, the suspension process that adds soda ash adopts milling treatment of colloid.Among the described step D, solid-liquid separation is by the double-effect evaporation device.
The silicate of described stablizer is any one or more mixture of water glass, water glass, potassium silicate; The solubility magnesium salts is one or more the mixture in sal epsom, magnesium chloride, the magnesium acetate; Phosphoric acid salt is one or more mixture such as tri-polyphosphate, trisodium phosphate, Sodium hexametaphosphate 99.
Because low polyalcohols is low-molecular-weight anion surfactant, too early joins in the reactor, in early stage because the shearing force under the motor rotation, centrifugal force, and the influence of temperature of reaction can have influence on its surfactivity.And the present invention joins low polyalcohols in the hydrogen peroxide, promptly hydrogen peroxide is carried out pre-treatment, and the process that makes its adding is to follow the adding of hydrogen peroxide to carry out simultaneously, makes low polyalcohols can both play effect in entire reaction.Hydrogen peroxide can slow down the decomposition of hydrogen peroxide after the pre-treatment through low polyalcohols, thereby has stablized the quality of product, the proportion of more effective control PC and stability.In addition, through repeatedly experiment, selected the rate of addition in suspension a and the hydrogen peroxide solution while dropwise reaction still to be: the volume ratio 1:1-3 of suspension a and hydrogen peroxide solution, the dropping time in described suspension a and the hydrogen peroxide solution while dropwise reaction still is 30-50 minute.The growth pattern that makes SPC-D of the present invention like this is the reunion formula, and the sodium percarbonate granules that crystallization goes out is loose, and proportion is lighter, dissolution rate and stable aspect all more common crystalline SPC-D increase.
On the other hand, when adding the suspension of soda ash, use colloidal mill equipment, make that the adding speed of soda ash is controlled, thereby make that the process of growth of SPC-D particle is controlled; By the double-effect evaporation device, remove redundant moisture at the unnecessary mother liquor of whole system, make raw materials such as wherein soda ash, salting-out agent obtain recycling, reduce consuming, avoided pollution simultaneously environment.
Embodiment
The preparation method of SPC-D of the present invention, concrete steps are:
1, the preparation of suspension a.In the water of 1000g, add a certain amount of yellow soda ash, salting-out agent, stablizer mixing successively, fully stir, be mixed with suspension a.Described weight ratio with yellow soda ash, salting-out agent, stablizer is 1:0.1-0.8:0.01-0.05.
Described salting-out agent can be sodium-chlor or sodium sulfate,
Described stablizer can be a silicate, and described silicate is any one or more mixture of water glass, water glass, potassium silicate; Also can be the solubility magnesium salts, described solubility magnesium salts be one or more the mixture in sal epsom, magnesium chloride, the magnesium acetate; Can also be phosphoric acid salt, described phosphoric acid salt be one or more mixture such as tri-polyphosphate, trisodium phosphate, Sodium hexametaphosphate 99.When being mixed with suspension a, the suspension process that adds soda ash preferably adopts milling treatment of colloid.
Following table is the specific embodiment of formulated suspension a:
| Embodiment | The yellow soda ash add-on | The salting-out agent kind | The salting-out agent add-on | Stabilizer type | The stablizer add-on |
| 1 | 100 grams | Sodium-chlor | 10 grams | Water glass | 1 gram |
| 2 | 100 grams | Sodium sulfate | 80 grams | Water glass | 5 grams |
| 3 | 100 grams | Sodium-chlor | 50 grams | Potassium silicate | 2 grams |
| 4 | 100 grams | Sodium sulfate | 60 grams | Water glass, waterglass mixture | 3 grams |
| 5 | 100 grams | Sodium-chlor | 70 grams | Sal epsom | 4 grams |
| 6 | 100 grams | Sodium sulfate | 40 grams | Magnesium chloride | 1.5 gram |
| 7 | 100 grams | Sodium-chlor | 20 grams | Magnesium acetate | 2.5 gram |
| 8 | 100 grams | Sodium sulfate | 30 grams | Sal epsom, magnesium chloride, magnesium acetate mixture | 3.5 gram |
| 9 | 100 grams | Sodium-chlor | 50 grams | Tri-polyphosphate | 4.5 gram |
| 10 | 100 grams | Sodium sulfate | 40 grams | Trisodium phosphate | 3 grams |
| 11 | 100 grams | Sodium-chlor | 35 grams | Sodium hexametaphosphate 99 | 2 grams |
| 12 | 100 grams | Sodium sulfate | 55 grams | Trisodium phosphate, Sodium hexametaphosphate 99 mixture | 2 grams |
2, the pre-treatment of hydrogen peroxide.In mass percentage concentration is to add low polyalcohols in the 25%-50% hydrogen peroxide, and the add-on of described low polyalcohols is the 0.05-1.0% of hydrogen peroxide quality.Described low polyalcohols for poly-hexylene glycol or poly-hexanol or poly-hexylene glycol and any one or more mixture.
Following table is the pretreated specific embodiment of hydrogen peroxide:
| Embodiment | Hydrogen peroxide concentration | The hydrogen peroxide add-on | Low polyalcohols kind | Low polyalcohols add-on |
| 1 | 25％ | 1000 grams | Poly-hexylene glycol | 1 gram |
| 2 | 50％ | 1000 grams | Poly-hexanol | 0.5 gram |
| 3 | 30％ | 1000 grams | Poly-hexylene glycol | 0.2 gram |
| 4 | 40％ | 1000 grams | The mixture of poly-hexylene glycol and poly-hexanol | 0.4 gram |
| 5 | 35％ | 1000 grams | The mixture of poly-hexanol and poly-hexylene glycol | 0.3 gram |
| 6 | 45％ | 1000 grams | Poly-hexylene glycol, poly-hexanol and poly-hexylene glycol mixture | 0.4 gram |
3, the preparation of mother liquor b.Get a certain amount of suspension a and a certain amount of through pretreated hydrogen peroxide, simultaneously in the dropwise reaction still, rate of addition is: suspension a and through the volume ratio 1:1-3 of pretreated hydrogen peroxide solution, described suspension a and the dropping time in pretreated hydrogen peroxide solution while dropwise reaction still are 30-50 minute, obtain mother liquor b;
Described in this step suspension a be 1:1 or 1:2 or 1:3 or 1:2.5 or 1:2.3 or 1:2.7 through the volume ratio of pretreated hydrogen peroxide; Rate of addition is: suspension a and through volume ratio 1:1 or 1:2 or 1:3 or 1:2.5 or the 1:2.3 or the 1:2.7 of pretreated hydrogen peroxide solution; The dropping time is 30 minutes or 50 minutes or 40 minutes.
4: ageing.With mother liquor b ageing 5-10 minute.The concrete time can be 5 minutes or 10 minutes or 7 minutes or 6 minutes.
5, solid-liquid separation.Mother liquor b after the ageing is handled by the double-effect evaporation device, separate out the SPC-D crystal,, the solid drying after separating is obtained the finished product SPC-D through solid-liquid separation.
The inventor has got 3 groups of finished product SPC-D that make according to the method described above, and is same, got 1 group of finished product SPC-D that adopts art methods to make, and the SPC-D that contrast obtains detects respectively, and the result is as follows:
| The project indicator | 1 group | 2 groups | 3 groups | The prior art contrast |
| Dissolution rate (second) | 36 | 35 | 39 | 60 |
| Wet stable % | 90.12 | 93.21 | 90.86 | 60-70 |
The dissolution rate testing method: use instrument numeral conductivitimeter, get in the distilled water of 2.5g sample adding 1000ml, measure its electric conductivity value under 4cm whirlpool condition, dissolution rate is 90% its maximum conductance value time corresponding.
Wet stability test method: use the constant damp heat test box of instrument, take by weighing 1.8g (0.0001g) sample and put into constant damp heat test box (the 40 ℃ ﹠amp that regulate in advance; 80%RH), measure its residual active oxygen after the week.
Claims (8)
1, a kind of preparation method of SPC-D, it may further comprise the steps:
A: yellow soda ash, salting-out agent, stablizer are mixed, be mixed with suspension a, described weight ratio with yellow soda ash, salting-out agent, stablizer is 1:0.1-0.8:0.01-0.05;
B: suspension a and hydrogen peroxide are added respectively in the reactor, and the volume ratio of described suspension a and hydrogen peroxide is 1:1-3, obtains mother liquor b;
C: with mother liquor b ageing 5-10 minute;
D: separate out the SPC-D crystal,, the solid drying after separating is obtained the finished product SPC-D through solid-liquid separation,
At salting-out agent described in the steps A is sodium-chlor or sodium sulfate, and described stablizer is silicate, solubility magnesium salts, phosphoric acid salt,
It is characterized in that among the described step B that the mode that suspension a and hydrogen peroxide are added respectively in the reactor is: described suspension a and hydrogen peroxide solution be simultaneously in the dropwise reaction still,
The hydrogen peroxide that adds among the described step B is for through pre-treatment, and the pre-treatment of described hydrogen peroxide is: add low polyalcohols in mass percentage concentration is the hydrogen peroxide of 25%-50%, the add-on of described low polyalcohols is the 0.05-1.0% of hydrogen peroxide quality.
2, SPC-D preparation method according to claim 1 is characterized in that the low polyalcohols that adds in the described hydrogen peroxide any one or more the mixture for poly-hexylene glycol or poly-hexanol or poly-hexylene glycol.
3, SPC-D preparation method according to claim 1, it is characterized in that the rate of addition in described suspension a and the hydrogen peroxide solution while dropwise reaction still is: the volume ratio 1:1-3 of suspension a and hydrogen peroxide solution, the dropping time in described suspension a and the hydrogen peroxide solution while dropwise reaction still is 30-50 minute.
According to claim 1 or 2 or 3 described SPC-D preparation methods, it is characterized in that in the described steps A that 4, when being mixed with suspension a, the suspension process that adds soda ash adopts milling treatment of colloid.
According to claim 1 or 2 or 3 described SPC-D preparation methods, it is characterized in that among the described step D that 5, solid-liquid separation is by the double-effect evaporation device.
6, SPC-D preparation method according to claim 1 is characterized in that at described silicate it being any one or more mixture of water glass, water glass, potassium silicate.
7, SPC-D preparation method according to claim 1 is characterized in that at described solubility magnesium salts be one or more mixture in sal epsom, magnesium chloride, the magnesium acetate.
8, SPC-D preparation method according to claim 1 is characterized in that at described phosphoric acid salt be one or more mixture such as tri-polyphosphate, trisodium phosphate, Sodium hexametaphosphate 99.
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| CNA2009100953961A CN101481090A (en) | 2009-01-08 | 2009-01-08 | Preparation method of sodium percarbonate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102642815A (en) * | 2012-03-05 | 2012-08-22 | 浙江金科过氧化物股份有限公司 | Circulatory recycling method of sodium percarbonate mother liquor |
| CN101786969B (en) * | 2010-01-29 | 2013-04-17 | 河北工业大学 | Method of joint production of urea hydrogen peroxide and sodium percarbonate |
| CN109824016A (en) * | 2019-03-25 | 2019-05-31 | 天津市郁峰化工有限公司 | A kind of production technology of calcium hypochlorite |
| CN111517287A (en) * | 2020-06-16 | 2020-08-11 | 中国水产科学研究院黄海水产研究所 | Production method of sodium percarbonate for aquaculture, product and application thereof |
| CN113582141A (en) * | 2021-08-02 | 2021-11-02 | 浙江金科日化原料有限公司 | Preparation method of sodium percarbonate with high stability and low micro calorific value |
-
2009
- 2009-01-08 CN CNA2009100953961A patent/CN101481090A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786969B (en) * | 2010-01-29 | 2013-04-17 | 河北工业大学 | Method of joint production of urea hydrogen peroxide and sodium percarbonate |
| CN102642815A (en) * | 2012-03-05 | 2012-08-22 | 浙江金科过氧化物股份有限公司 | Circulatory recycling method of sodium percarbonate mother liquor |
| CN109824016A (en) * | 2019-03-25 | 2019-05-31 | 天津市郁峰化工有限公司 | A kind of production technology of calcium hypochlorite |
| CN111517287A (en) * | 2020-06-16 | 2020-08-11 | 中国水产科学研究院黄海水产研究所 | Production method of sodium percarbonate for aquaculture, product and application thereof |
| CN113582141A (en) * | 2021-08-02 | 2021-11-02 | 浙江金科日化原料有限公司 | Preparation method of sodium percarbonate with high stability and low micro calorific value |
| CN113582141B (en) * | 2021-08-02 | 2023-11-24 | 浙江金科日化新材料股份有限公司 | Preparation method of sodium percarbonate with high stability and low trace heat value |
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